Category: 2033-24-1

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2033-24-1 as follows. Formula: C6H8O4

A solution of 2,2-dimethyl-1,3-dioxane-4,6-dione (10.0g, 69.4mmol) disolved in trimethoxymethane (40mL, 366mmol) was refluxed at 110C for 3 hours.Then the reaction mixture was cooled to room temperatue and yellow crystalformed, the crystal was filtered out, washed with petroleum ether and dried in the air to give the titled compound as a light yellow crystaline solid (7.5g,59%). 1H NMR (400 MHz, Chloroform-d) delta 8.15 (s, 1H), 4.27 (s, 3H), 1.72(s, 6H).

According to the analysis of related databases, 2033-24-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Cheng, Yu; Shen, Jian; Peng, Run-Ze; Wang, Gui-Feng; Zuo, Jian-Ping; Long, Ya-Qiu; Bioorganic and Medicinal Chemistry Letters; vol. 26; 12; (2016); p. 2900 – 2906;,
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These common heterocyclic compound, 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. category: esters-buliding-blocks

General procedure: Method A: Adapted from the procedure of Srensen et al.14 To a solution of Meldrum?s acid (1equiv) in dichloromethane at 0C was added pyridine (2equiv) drop wise, and the resulting solution was stirred for 15min. The corresponding acid chloride (1equiv) was added to this reaction mixture. Thereafter, the reaction was stirred for 1.5h at 0C, and for an additional 1.5h at room temperature. The reaction was quenched with 2M hydrochloric acid, and extracted with dichloromethane. The combined organic layers were dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography using a gradient from 5% to 10% ethyl acetate in hexane, 1% acetic acid to yield acyl Meldrum?s acids (11a-e, j, l, p).

The synthetic route of 2,2-Dimethyl-1,3-dioxane-4,6-dione has been constantly updated, and we look forward to future research findings.

Reference:
Article; Verma, Astha; Wong, Dawn M.; Islam, Rafique; Tong, Fan; Ghavami, Maryam; Mutunga, James M.; Slebodnick, Carla; Li, Jianyong; Viayna, Elisabet; Lam, Polo C.-H.; Totrov, Maxim M.; Bloomquist, Jeffrey R.; Carlier, Paul R.; Bioorganic and Medicinal Chemistry; vol. 23; 6; (2015); p. 1321 – 1340;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione, belongs to esters-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2033-24-1, Recommanded Product: 2033-24-1

2,4,5-Trifluorophenylacetic acid (2-1) (available from several commercial supplers) (25 g, 0.132 mol), Meldrum’s acid (21 g, 0.145 mol), and DMAP (1.29 g, 0.0011 mol) were charged into a 1000 mL three-neck flask. Acetonitrile (75 mL) was added in one portion at room temperature. N,N-diisopropylethylamine (49.2 mL, 0.283 mol) was added in one portion at room temperature while maintaining the temperature below 40 C. Pivaloyl chloride (17.8 mL, 0.145 mol) was added dropwise over 1 to 2 h while maintaining the temperature below 50 C. The reaction was aged at 45-50 C for 2-3 h and cooled to 0 C. 1N HCl (300 mL) was added dropwise over 1 h while the Meldrum’s adduct 2-2 was crystallized out. The product was collected by filtration and washed with 20% MeCN/ water. After drying, 36.5 g of the Meldrum’s acid adduct was obtained (88% yield). 1H-NMR (400 MHz, CDCl3): delta 15.50 (s, 1H), 7.14 (m, 1H), 6.96 (m, 1H), 4.45 (s, 2H), 1.76 (s, 6H) ppm. 13C-NMR (100 MHz, CDCl3): delta 192.76, 170.66, 160.42, 156.47 (ddd, J CF = 245.7, 9.6, 2.4 Hz), 149.79 (ddd, J CF = 251.4, 14.5, 12.0 Hz), 146.90 (ddd, J CF = 244.9, 12.0, 3.2 Hz), 119.40 (dd, J CF = 19.3, 5.6 Hz), 117.41 (ddd, J CF = 18.5, 5.6, 4.0 Hz), 105.80 (dd, J CF = 28.1, 20.9 Hz), 105.63, 91.99, 34.59, 27.06 ppm.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; MERCK & CO., INC.; WO2004/83212; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 2033-24-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Pyridine (2 equiv) was added to a solution of Meldrum?s acid (1 equiv) in DCM (0.7 M). The acyl chloride (1 equiv) was dissolved in DCM (1.4 M) and was added dropwise to the Meldrum?s acid solution at 0 C. The reaction was stirred for 1.5 h at 0 C and 1.5 h at room temperature. An additional portion acyl chloride (0.5 equiv) was added and stirring was continued for 12 h at room temperature. Then the reaction was stopped by adding HCl (2 M) and diluted with DCM. The organic phase was separated, dried over Na2SO4 and evaporated. The crude product was either purified by column chromatography or crystallized to yield the pure acyl Meldrum?s acid.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2,2-Dimethyl-1,3-dioxane-4,6-dione, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Beyer, W.R. Christian; Woithe, Katharina; Lueke, Bettina; Schindler, Michael; Antonicek, Horst; Scherkenbeck, Juergen; Tetrahedron; vol. 67; 17; (2011); p. 3062 – 3070;,
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Ester – an overview | ScienceDirect Topics

Application of 2033-24-1,Some common heterocyclic compound, 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione, molecular formula is C6H8O4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

2,4,5-Trifluorophenylacetic acid (2-1) (11.4 g, 60 mmol) was dissolved in THF (60 mL) and 1,1′-carbonyldiimidazole (10.7 g, 66 mmol) was added over 5 min. The mixture was warmed to 51 C, Meldrum’s acid (9.51 g, 66 mmol) was added, and the mixture was aged for 3 h. The reaction mixture was diluted with IPAc (60 mL) and water (60 mL), and the pH was adjusted to 2.4 with concentrated hydrochloric acid (11.5 mL). The aqueous layer was separated, and the orgnic layer was washed at 36 C with 0.1 N HCl (60 mL). The organic layer was concentrated, flushed with IPAc, and the residue was slurried in 2:1 heptane/IPAc (70 mL). the mixture was cooled over an ice-bath, then filtered, rinsing the solid with 2:1 heptane/IPAc. After drying, the Meldrum’s acid adduct was obtained as a solid (15.1 g) in 80% yield. The Meldrum’s acid adduct (22.1 g, 70 mmol) and the triazole hydrochloride 1-4 (16.0 g, 70 mmol) were sluuried in IPAc (220 mL) and N,N-diisopropylethylamine (12.8 mL) was added. After aging for 3.5 h at 85 C, water (175 mL) was added and the mixture was transferred to a separatory funnel with a 40-mL rinse with IPAc. The aqueous layer was separated and the organic layer was washed with water (100 mL). The organic layer was partially concentrated under reduced pressure to give a 65 g of solution of the ketoamide 2-3 in IPAc. n-Heptane (30 mL) was added at roo temperature, followed by seed crystals of ketoamide. Additional heptane (20 mL) was added dropwise, and the mixture was stirred overnight. Additional heptane (50 mL) was added slowly and after aging for 2 h, the solids were filtered and washed with 2.2:1 heptane/IPAc (30 mL). After drying, the ketoamide 2-3 was obtained in 92% yield (26.3 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2-Dimethyl-1,3-dioxane-4,6-dione, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2004/83212; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione, belongs to esters-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2033-24-1, category: esters-buliding-blocks

2,4,5-trifluorophenylacetic acid (30 g), tetrahydrofuran (360 ml_), 1 ,1 -carbonyl diimidazole (25.5 g) at about 5O0C, and meldrums acid (22.7 g) are combined. The mixture is stirred for about five hours at the same temperature. The reaction mass is then cooled to about 3O0C. Isopropyl acetate (180 ml_) and water (180 ml_) are added and stirred for about 30 minutes. The reaction mass is cooled to about O0C and pH is adjusted to about 2.4 using 36% aqueous hydrochloric acid. The organic layer is separated, washed with 0.1 N aqueous hydrochloric acid and distilled off completely. To the residue obtained, n-heptane (140 ml_) and isopropyl acetate (70 ml_) are charged at about 3O0C and stirred at about O0C for about 90 minutes. The separated solid is filtered and washed with a mixture of n-heptane (20 ml_) and isopropyl acetate (10 ml_). The wet cake is dried at about 5O0C for about 4 hours to afford the title compound. (Yield: 60.1 %; purity by HPLC: 98.0%)

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; DR. REDDY’S LABORATORIES LIMITED; DR. REDDY’S LABORATORIES, INC.; WO2009/85990; (2009); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

2033-24-1,Some common heterocyclic compound, 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione, molecular formula is C6H8O4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Meldrum’s adduct (19)2,4,5-Trifluorophenylacetic acid (500.0 gm, 2.63 mol) (18) was suspended in tetrahydrofuran (5.26 vol, 2.63 Ltr) at 25-30C and the reaction mixture was stirred for 10- 15 minutes. To this clear solution, l,r-carbonyldmidazole (1.5 eq, 639.68 gm) was charged in four lots and the reaction mixture was stirred for 2-3 hours at 25-300C. After 2- 3 hours stirring, Meldrum’s acid (1.2 eq, 454.87 gm) was charged and the reaction mixture was heated for 6 hours at 50-550C. After 6 hours heating at 50-55C, the tetrahydrofuran was distilled out completely at 50-55C under reduced pressure to give a dark yellow coloured residue. The dark yellow residue was acidified by using a 1:1 mixture of 35% hydrochloric acid : water (0.5 vol, 250.0 ml) at 0-50C. The product was extracted from the aqueous solution by using dichloromethane (3 x 5.0 vol, 3 x 2.5 Ltr). The combined dichloromethane layers were further washed with water (3 x 10.0 vol, 3 x 5.0 Ltr). After water washing, the dichloromethane was completely distilled under reduced pressure to give a dark yellow fluffy solid. The product was further washed with methanol (2.0 vol, 1.0 Ltr) at 0-50C.Molar Yield: 60-65% (505.0 gm) Chemical Purity: 98-99.5% (as measured by HPLC)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2033-24-1, its application will become more common.

Reference:
Patent; GENERICS [UK] LIMITED; MYLAN INDIA PRIVATE LIMITED; GORE, Vinayak Govind; GADAKAR, Maheshkumar; BHOSLE, Priyanka; SHINDE, Suresh; WO2010/131025; (2010); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 2033-24-1, name is 2,2-Dimethyl-1,3-dioxane-4,6-dione, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 2033-24-1

The Meldrum’s acid [1] (50.0 g, 347 mmol) and trimethyl orthoformate [2] (184 g) were charged into a 500 mL four-necked flask and heated under reflux for 1 hour. After completion of the reaction, the solvent was removed by an evaporator, and the crude product was recrystallized in a hexane / tetrahydrofuran mixed solvent to give 43.7 g of the compound [66] (yield: 68%).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 2033-24-1.

Reference:
Patent; NISSAN CHEMICAL INDUSTRIES, LTD.; MINAMI, SATOSHI; (157 pag.)TWI588139; (2017); B;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics